BATCH DISTILLATION

In Partial Fulfilment of the Requirements for the Course

Chemical Engineering Laboratory 1 for Chemical Engineering

Submitted by:
Benito, Angelica
Bose, Judy Ann
Decena, Christrian
Lim, Van Jansen
Maquera, Kricel-Mae

Submitted to:
ENGR. CAESAR P. LLAPITAN

MAY, 2018
ABSTRACT
 TABLE OF CONTENTS
I. Introduction ........................................................................................................................ 1

II. Objectives .......................................................................................................................... 1

III. Theory ............................................................................................................................. 1

A. Rectangular Notch ..................................................... Error! Bookmark not defined.

B. Triangular Notch ....................................................... Error! Bookmark not defined.

C. Applications ................................................................................................................ 4

IV. Description of Apparatus ................................................................................................ 4

V. Experimental Procedures ................................................................................................... 8

A. General Start-up Procedures...................................... Error! Bookmark not defined.

B. General Shut Down Procedures ................................ Error! Bookmark not defined.

C. Equipment Set-up Procedures ................................... Error! Bookmark not defined.

VI. Results and Discussion ................................................................................................... 8

VII. Conclusion .................................................................................................................... 10

VIII. Recommendation ....................................................................................................... 11

IX. Appendices .................................................................................................................... 11

A. Principles ................................................................... Error! Bookmark not defined.

1. For the Rectangular Notch ..................................... Error! Bookmark not defined.

2. For the V-notch Weir ............................................. Error! Bookmark not defined.

B. Calculations ............................................................................................................... 11

X. References ........................................................................................................................ 15
 NOMENCLATURE

m Mass of the solution

v Volume of the solution
 Density
%wt Mass fraction
SG Specific gravity
 I. Introduction
Distillation is a process that separates mixtures by selective boiling and condensation.
Distillation results from either completely separating the mixture or partial separation of the
mixture, resulting in the increase of concentration of a selected component. Distillation
operates under the principle of relative volatility or boiling points. The process involves
production of vapour by boiling the liquid mixture in a still and removal of the vapour from
the still by condensation. Due to differences in relative volatility or boiling points. The
vapour is rich in light components and the liquid is rich in heavy components.

In batch distillation, the mixture is separated into its components before the distillation of
the still is changed again. It is in contrast with continuous distillation where the feedstock is
continuously fed without interaction. It is the oldest operation used for separation of liquid
mixtures. It is also widely used for the production of fine chemicals and specialized products.

In this experiment Batch distillation method is used to concentrate the mixture of ethanol
and water up to 10%of ethanol. The experiment aims to increase the initial concentration of
ethanol in water until the distillate reaches 40 mL in the beaker. The 40 mL of the distillate
will be collected before the distillation process ended. The chemical and thermodynamic
properties are also gathered as data for the calculation of the concentration of distillates.

II. Objectives
The objective of this experiment is to apply the process of distillation to a mixture of
ethanol and water to obtain a new mixture with an increased concentration of ethanol.
Specifically, it aims to:
1. Calculate the number of moles of ethanol and water in the initial flask, the three
distillate samples and the final mixture.
2. Calculate the mass fraction of ethanol in the three distillate samples and the final
mixture.
3. Approximate the x-T curve using the distillate samples in the ethanol-water calculated
value.

III. Theory
The simplest form of batch distillation consists of a heated vessel (pot or boiler), a
condenser, and one or more receiving tanks. No trays or packing is provided. Feed is charged
into the vessel and brought to boiling. Vapors are condensed and collected in a receiver. No

1
reflux is returned. The rate of vaporization is sometimes limited to prevent “bumping” the
charge and to avoid overloading the condenser, but other controls are minimal. This process
is often referred to as a Rayleigh distillation.

THERMOMETER

WATER OUTLET

DISTILLING FLASK CONDENSER

MIXTURE

DISTILLATE

COLD WATER INLET

Figure 1: Simple Batch Distillation

In batch distillation, the more volatile component is evaporated from the still which
therefore becomes progressively richer in the less volatile constituent. Distillation is
continued, either until the residue of the still contains a material with an acceptably low
content of the volatile material, or until the distillate is no longer sufficiently pure in respect
of the volatile content.

For example, consider a mixture consisting of two components, A and B, which have
boiling points of 70°C and 100°C, respectively. When the mixture begins to boil, the vapor
phase that is formed will be richer in A than the liquid phase. This is because A has a lower
boiling point and vaporizes more easily than B. Therefore, A has a greater tendency to enter
the vapor phase while B tends to remain in the liquid phase. Of course, if the entire mixture
could boil away, the resulting vapor would have the same concentration of A and B as the
original liquid mixture. However, if only a fraction of the liquid can boil, the vapor will
contain a higher concentration of A than the original liquid mixture.

As the mixture continues to boil, the compositions of both the vapor and liquid phases
change with time. Since A enters the vapor phase more quickly than B, the concentration of
A in the liquid phase decreases while that of B increases. Also, as the temperature of the

2
boiling liquid increases, more B vaporizes as time passes, and the concentration of B in the
vapor phase also increases with time.

If some fraction of the original mixture vaporizes and the vapor is collected and allowed
to cool and condense in a separate container, the new liquid mixture (first distillate) will have
a higher concentration of A than the original did. If the first distillate is distilled by repeating
the process, a second distillate with an even higher concentration of A will be obtained. This
is basically how distillation works. It is just a series of vaporization and condensation
processes that continues until a desired concentration is reached.

In general, an equilibrium stage in any type of unit operation process is defined as an area
in which different phases are brought into close contact so that a component can be
redistributed between the phases to equilibrium concentrations. In the simple batch
distillation setup in this experiment, liquid in the 1000-mL flask is in close contact with the
vapor phase that forms as the mixture boils, and this is the only place where this situation is
present in the setup. Therefore, there is one equilibrium stage in this batch distillation.
Assuming everything works ideally, the vapor phase is in equilibrium with the liquid in the
flask at any given time.

The type of equilibrium information that is needed for analyzing this separation process is
that which shows the vapor-liquid equilibrium relationship for an ethanol/water mixture.

3
 1

0.9

Mole Fraction A in Vapor 0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Mole Fraction A in Liquid

Figure 2: Ethanol-Water Equilibrium Curve

The most useful representation of the data is a y versus x graph, where y and x are the
vapor and liquid phase concentrations, respectively, of the more volatile component, ethanol.
Points on the curve depicted in such a graph represent the concentration of ethanol in the
vapor and liquid phases at equilibrium. Along the equilibrium curve, pressure is constant, but
temperature is different at each point. Figure 2 depicts the y versus x graph ethanol and water.

A. Applications
In several chemical engineering applications, weirs are commonly used to either
regulate or to measure the volumetric flow rate of liquids. They are elevated structures
that are used to control outflow and/or measure flow from basins and drainage channels.
They are often used in open channel hydraulics such as water supply, wastewater and
sewage systems. Broad-crested weirs can be observed in dam spillways where the broad
edge is beneath the water surface across the entire stream. Flow measurement
installations with broad-crested weirs will meet accuracy requirements only if they are
calibrated.

IV. Description of Apparatus

A. Main Apparatus
Table 1: List of Apparatus needed in Batch Distillation

LEGEND APPARATUS DESCRIPTION

4
 1 Distilling flask is used to separate tow liquid with
different boiling points. The flask typically
Distilling flask with
consists of a sphere-shaped base, a narrow
Rubber Stopper neck, and a side-arm tube, with the top of
the flask neck sealed with a cork or rubber
stopper.
2 Laboratory thermometers are used to measure
temperatures or temperature changes with a
Thermometer high degree of precision. They are made of
metal or glass and strengthened through
thermal tempering or annealing.
3 A condenser is a device used in to cool
hot steam into liquids. It is a long, circular glass tube.
Condenser Inside the tube there is another, smaller tube. The hot
gas goes through the smaller, inside tube, while in the
outside one cold water goes around.
4 Rubber tubing is used in flow lines for fluids and gases in
a variety of hydraulic, pneumatic, process, medical, and
Latex Tubing specialty applications. Rubber tubing is flexible and
resilient due to its natural or synthetic rubber
construction.
5 Copper tubing is most often used for supply of hot and
cold tap water, here are two basic types of copper
tubing, soft copper and rigid copper. Copper tubing is
Copper Tubing joined using flare connection, compression
connection, or solder. Copper offers a high level
of corrosion resistance.
6 Gas Stove is uysed as a source of heat to boil the
Gas Stove
mixture
7 Iron stand and Iron clamp is used to hold the
Iron stand and Iron
apparatus in their appropriate position for the
Clamp
exzperiment
8 Plastic collection Container used to collect the distillate.
bottles, 40 mL

Batch Distillation Setup:

5
 Figure 3: Flow Over Weirs – Rectangular Weir

B. Other Apparatus
[1] Stopwatch
 It is used for measuring the amount of time of a certain activity.

Figure 4: Stopwatch

[2] Erlenmeyer Flask

 It is used as a container for the preparation of the mixture

6
[3] Beaker
 It is used to collect and measure the distillate

[4] Wire Gauze

 It is used to support the distillation flask during the heating of the mixture.

[5] Analytical Balance

 It is used to measure the weights of the Beaker and other apparatus as well as
the solution during the preparation.

[6] Graduated Cylinder

 It is used to measure the components for the preparation of the mixture

7
 [7] Pipette and Aspirator
 It is used to accurately measure the ethanol to be used iun preparing the

mixcture

[8] Ethanol Solution 95% by volume

 It is used as one of the component of the mixture

V. Experimental Procedures
First, label the three plastic distillate collection bottles and make a mark to indicate the
level equal to 40mL. Then pour 40 mL of the initial 30% ethanol in water solution into a 50
mL graduated cylinder. Since specific gravity is dependent upon temperature, measure the
temperature of the solution. Once the specific gravity and temperature have been determined,
the solution may be discarded.

Second, determine the weight of an empty 1000-ml flask. Then add 500 mL of the initial
10% ethanol in water solution to the 1000 –mL distilling flask and determine the weight of
the flask and solution. Be certain that distillation apparatus has been set up correctly and that

8
you understand how the system operates. Place the rubber stopper (with the copper tubing in
it) on the flask that contains the solution. The tubing should stick out past the stopper
approximately ½” into the flask. Do not force the thermometer or copper tubing into the
rubber stopper. Afterwards, start flowing the water through the cooling jacket of the
condenser. Make sure that the flow is from bottom to top otherwise, the coils may not be
fully bathed in the cooling water. The flow should be a gentle, steady stream. Be certain that
the rubber tubing is not resting on or near the gas stove since the smell of burning rubber is
not pleasant.

Third, turn the gas stove setting to medium-high and leave it at this setting for
approximately 10 minutes, or so until the solution starts to boil. Then turn the heat setting to
medium. The solution should begin to boil within 8-10 minutes. Once the solution begins to
boil, it should be about 3-5 minutes until you observe distillate dripping into the collection
bottle. Throughout the experiment, ensure that the boil is very gentle. After the first bottle has
collected 40 mL of distillate, quickly replace it with an empty one. This needs to be done as
rapidly as possible so that minimal distillate is lost. Next, cover and label the bottle
containing the first distillate sample. Record the temperature of the vapor phase above the
boiling solution. Also determine the mass of the first distillate sample. This will be used to
calculate the specific gravity of the first distillate. The temperature, density, mass fraction
correlation chart only goes up to 40°C. Therefore, if the distillate is warmer than 40°C, you
will need to allow it to cool before measuring its specific gravity. If it is already cool enough,
it is a good idea to go ahead and calculate its specific gravity while collecting the second
distillate sample. Subsequently, pour your distillate into a 50-mL cylinder. If the cylinder is
too full, some of the liquid can be poured out after the mass is measured since it is not
necessary to have the total sample present to measure specific gravity; specific gravity is not
dependent on sample size. Recall that the objective is to deduce the number of moles each of
water and ethanol in each of your distillate samples so that you can carry out a final mass
balance.

Lastly, repeat the procedure by collecting the second and third distillate sample. Once you
are close to collecting 40 mL of the third distillate, turn the gas stove off and carefully
remove the flask from on top of the gas stove. Do not remove the distillate collection bottle
until the mixture in the flask has stopped boiling for about 5 minutes. This helps to ensure
that no vapors remain in the tubing. After the third distillate collection bottle has been

9
 removed, the flask can be removed from the clamp, and the stopper/tubing apparatus can be
detached. However, be sure to keep the flask covered while it is cooling so that no vapors
escape. The flask mixture will need to cool quite a bit before its specific gravity can be
measured. A cool water bath will help expedite the cooling process of the flask mixture. In
addition, gently swirl the liquid in the flask, this will help release heat more quickly. Once the
solution in the flask has cooled to below 40°C, determine the mass of the solution that
remains in the flask. Calculate its specific gravity of the solution remaining in the flask using
the same method you used for the initial solution. For each of your samples, use the specific
gravity, temperature and Table of the Densities of ethyl alcohol (C2H5OH in water) (Perry
2008) to determine the mass percentage of ethanol in each sample. You may need to use
bilinear interpolation to calculate these values.

VI. Results and Discussion

VII. Conclusion
One of the objectives of this experiment was to determine the characteristics of a
rectangular notch and a triangular (V) notch. On the rectangular notch, there is a slight
downward curve in the graph between log H and log Q. From this, we can conclude that the
Cd that will also be affected. According to the theory of rectangular notch discussed in
Chapter III.A., the discharge from the rectangular notch will be considerably less,
approximately 60% of the theoretical analysis due to curvature effects. This means that
during the experiment, the flow of water through the notch is not parallel and not normal to
the plane of the weir. Due to viscosity and surface tension, the free surface didn’t remain
horizontal to the plane of the weir. The result is that the shape of the nappe as it passes
through the notch will form a curvature, the width of it reduced due to the contraction at each
end.

In the flow over triangular notch, a 90o V-notch weir was used. According to the theory,
this notch is used for lower discharges at a given H, although in this experiment, the H is not
given but rather it was determined. Instead, it was the volume who has a constant value of
0.05 m3. Generally, the discharge coefficients that must be obtained in v-notch weir are lower
than the rectangular notch. This was proven to be true in this experiment since they are lower
than the rectangular notch. Note that the shape of the nappe does not change with the head H,

10
 giving greater measurement accuracy compared to the rectangular notch. This also causes the
coefficient of discharge to not vary so much with the head H.

In general, for applications where lower discharges are needed at a given height of the
free surface of water above the notch base, the V-notch weir should be used. The V shape
also means that they are more sensitive at low flows, but the width increases to accommodate
larger flows. On the other hand, the rectangular weir is best applied for large heads and a low
velocity of approach in the weir channel. Hence it is best used for larger flows because the
width can be chosen so that it can pass the expected flow at a suitable depth.

VIII. Recommendations
Preparing the 10% solution must be more precise to obtain an accurate mixture of ethanol
and water solution. The apparatus should be calibrated to have accurate result. Also, some of
the evaporated water may be escaped from the process due to the error in settling the
apparatus therefore, the distillation set-up must operate correctly. No broken apparatus used
and it must be free from dirt.
IX. Appendices
A. Calculating the number of moles of ethanol and water in the initial flask, the three
distillate samples and the final mixture.
Chemical engineers typically perform mole balance analyses on processes as a means of
checking to see that all material is accounted for. In general, this means checking to see that
Input – Generation – Output – Consumption = Accumulation
In this experiment, the mole balance can be thought of in terms of
Moles in original flask mixture = -Moles in Distillate 1 – Moles in Distillate 2 + Moles in
Distillate 3 + Moles in the final flask mixture
 1mol   1mol   1mol   1mol   1mol 
457.37 g     35 g    36.28 g    37.05 g    565.7 g  
 52 g   52 g   52 g   52 g   52 g 
8.7955 moles  8.7955 moles
B. Calculating the mass fraction of ethanol in the mixture
Using bilinear interpolation formula,

(x 2  x)(y 2  y) (x  x 1 )(y 2  y) (x 2  x)(y  y 1 ) (x  x 1 )(y  y 1 )

P (Q 11 )  (Q 12 )  (Q 21 )  (Q 22 )
(x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 )
The specific gravity, temperature and Table of the Densities of ethyl alcohol (ethanol –

11
C2H5OH) are given in Perry’s Chemical Engineering Handbook to determine the mass
percentage of ethanol in each sample.
1. Initial Flask Mixture
At T = 30°C;  =0.94922, %wt = 29

At T = 35°C;  =0.94590, %wt = 29

At T = 30°C;  =0.94741, %wt = 30

At T = 35°C;  =0.94403, %wt = 30

Solving for y,

(x 2  x)(y 2  y) (x  x 1 )(y 2  y) (x 2  x)(y  y 1 ) (x  x 1 )(y  y 1 )

P (Q 11 )  (Q 12 )  (Q 21 )  (Q 22 )
(x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 )

(35 - 33)(30 - y) (33  30)(30  y) (35 - 33)(y - 29)

0.943  (0.94922) (0.94741) (0.94590)
(35  30)(30  29) (35  30)(30  29) (35  30)(30  29)
(33  30)y  29)
 (0.94403)
(35  30)(30  29)

y  30.55%

2. 1st distillate sample

At T = 35°C;  =0.87615, %wt = 61
At T = 40°C;  =0.87180, %wt = 61
At T = 35°C;  =0.8739, %wt = 62
At T = 40°C;  =0.86943, %wt = 62

Solving for y,

(x 2  x)(y 2  y) (x  x 1 )(y 2  y) (x 2  x)(y  y 1 ) (x  x 1 )(y  y 1 )

P (Q 11 )  (Q 12 )  (Q 21 )  (Q 22 )
(x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 )

12
 (40 - 36)(62- y) (36  35)(62  y) (40 - 36)(y - 61)
0.875  (0.87615) (0.87180) (0.87390)
(40  35)(62  61) (40  35)(62  61) (40  35)(62  61)
(36  35)y  61)
 (0.86943)
(40  35)(62  61)
y  61.123%
3. 2nd Distillate Sample

At T = 30°C;  =0.90805, %wt = 49

At T = 35°C;  =0.90396, %wt = 49

At T = 30°C;  =0.90580, %wt = 50

At T = 35°C;  =0.90168, %wt = 50

Solving for y,

(x 2  x)(y 2  y) (x  x 1 )(y 2  y) (x 2  x)(y  y 1 ) (x  x 1 )(y  y 1 )

P (Q 11 )  (Q 12 )  (Q 21 )  (Q 22 )
(x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 )

(35 - 33.5)(50- y) (33.5  30)(50  y) (35 - 33.5)(y - 49)

0.875  (0.90805) (0.90396) (0.90580)
(35  30)(50  49) (35  30)(50  49) (435  30)(62  61)
(33.5  30)(y  49)
 (0.90168)
(35  30)(50  49)

y  49.005%
4. 3rd Distillate Sample

At T = 30°C;  =0.92979, %wt = 39

At T = 35°C;  =0.91597, %wt = 39

At T = 30°C;  =0.91770, %wt = 40

At T = 35°C;  =0.91385, %wt = 40

Solving for y,

13
 (x 2  x)(y 2  y) (x  x 1 )(y 2  y) (x 2  x)(y  y 1 ) (x  x 1 )(y  y 1 )
P (Q 11 )  (Q 12 )  (Q 21 )  (Q 22 )
(x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 )

(35 - 34)(40- y) (34  30)(40  y) (35 - 34)(y - 39)

0.875  (0.92979) (0.91597) (0.91770)
(35  30)(40  39) (35  30)(40  39) (35  30)(40  39)
(34  30)(y  49)
 (0.91385)
(35  30)(40  39)
y  39.96%
5. Final Flask Mixture

At T = 35°C;  =0.95973, %wt = 21

At T = 40°C;  =0.95687, %wt = 21

At T = 35°C;  =0.95809, %wt = 22

At T = 35°C;  =0.95516, %wt = 22

Solving for y,

(x 2  x)(y 2  y) (x  x 1 )(y 2  y) (x 2  x)(y  y 1 ) (x  x 1 )(y  y 1 )

P (Q 11 )  (Q 12 )  (Q 21 )  (Q 22 )
(x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 )

(40 - 39)(22- y) (39  35)(22  y) (40 - 39)(y - 21)

0.875  (0.95973) (0.95687) (0.95809)
(40  35)(22  21) (40  35)(22  21) (40  35)(22  21)
(39  35)(y  21)
 (0.95516)
(40  35)(22  21)
y  21.932%

14
 C. Documentations

Figure 5: V-notch weir experiment

Figure 6: Rectangular Notch Experiment

X. References
[1] Mutjaba, I. (n.d.). Batch Distillation Design and Operation (Vol. 3). Imperial College
Press.
[2] Wankat, P. C. (2007). Separation Process Engineering Includes Mass Transfer
Analysis, Third Edition.
[3] R.H. Perry, C.H Chilton, and S.O. Kirkpatrick (Eds.), Chemical Engineers Handbook,
8th ed., New York, McGraw-Hill, p. 2-117, p. 13, 2008

15
[4] Liu, S. X., & Ming, P. (2009). The Simulation of Simple Batch Distillation of
Multiple Component Mixtures via Rayleigh's Equation. Wiley Interscience, 7.

16